A poly (N-isopropyl acrylamide) (polyNIPA)-based hybrid column for capillary liquid chromatography (cLC) was prepared with N-isopropyl acrylamide (NIPA) and alkoxysilanes through a sol–gel “one-pot” method. In this process, the hydrolyzed tetramethoxysilane (TMOS) and vinyltrimethoxysilane (VTMS) were the precursors for the synthesis of a silica-based monolith and subsequently reacted with organic monomer (NIPA) via free radical polymerization within the confines of a capillary. The effects of polymerization temperature, the volume of TMOS, VTMS, and acetic acid (HAc) as well as the amount of progens [polyethylene glycol 10,000 (PEG10000) and urea] on the morphology and permeability were investigated in detail. Uniform pore structure and good mechanical stability were obtained for columns prepared under optimized conditions. Separation of various neutral, acidic and basic analytes was achieved by cLC in reversed-phase liquid chromatography (RP-LC) mode. Moreover, the resulting hybrid column was also applied for the analysis of small organic pollutants, including polycyclic aromatic hydrocarbons (PAHs), perfluorinated compounds (PFCs) and chlorophenols (CPs). The successful application demonstrated its potential in the separation of small molecules.

中文翻译：

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制备聚（N-异丙基丙烯酰胺）混合柱的溶胶-凝胶法及其在毛细管液相色谱小分子分析中的应用

使用 N-异丙基丙烯酰胺 (NIPA) 和烷氧基硅烷通过溶胶-凝胶“一锅法”制备了用于毛细管液相色谱 (cLC) 的聚 (N-异丙基丙烯酰胺) (polyNIPA) 混合柱。在此过程中，水解的四甲氧基硅烷 (TMOS) 和乙烯基三甲氧基硅烷 (VTMS) 是合成二氧化硅基整料的前体，随后在毛细管范围内通过自由基聚合与有机单体 (NIPA) 反应。详细研究了聚合温度、TMOS、VTMS 和乙酸 (HAc) 的体积以及前体 [聚乙二醇 10,000 (PEG10000) 和尿素] 的量对形态和渗透性的影响。在优化条件下制备的色谱柱获得了均匀的孔结构和良好的机械稳定性。在反相液相色谱 (RP-LC) 模式下，通过 cLC 实现了各种中性、酸性和碱性分析物的分离。此外，所得混合色谱柱还用于分析小有机污染物，包括多环芳烃 (PAH)、全氟化合物 (PFC) 和氯酚 (CP)。成功的应用证明了其在小分子分离方面的潜力。